农药学学报2017，Vol.19Issue(4)：482-490,9.DOI:10.16801/j.issn.1008-7303.2017.0063
液相色谱-串联质谱法同时测定菠菜、土壤及水体中螺虫乙酯及4种代谢物残留
Simultaneous determination of spirotetramat and its four metabolites in Spinacia oleracea L., soil and water using liquid chromatography-tandem mass spectrometry
摘要
Abstract
A rapid and sensitive method based on QuEChERS and solid phase extraction using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative ion scanning and multiple reaction monitoring (MRM) mode was developed for the residue detection of spirotetramat and its four metabolites (B-enol, B-keto, B-mono and B-glu) in Spinacia oleracea L., soil and water. When using aqueous phase of acetonitrile-0.5% formic acid as the mobile phase, gradient elution resulted in the best chromatographic resolution and sensitivity. When 0.1% formic acid-acetonitrile solution was used as the extraction solvent and the samples was purified by 50 mg m (PSA) : m (GCB) = 1 : 1, at the fortification levels of 0.05, 0.5 and 1mg/kg, the recoveries of spirotetramat and its four metabolites in spinach and soil were 81%-103% and 82%-98%, the RSD were 1.7%-7.9% and 1.9%-7.6%, respectively. The recoveries of spirotetramat and its four metabolites in water was 82%-95%, the RSD was 1.5%-6.2%, at the fortification levels of 0.005, 0.05 and 0.5 mg/L when the NH2 column was used as the solid phase extraction column and 10 mL of dichloromethane was used as the elution solvent. At concentrations ranging from 0.002-1 mg/L, there were good linear relationships between the mass concentration of spirotetramat and its four metabolites and the corresponding peak area, the correlation coefficients (r) were in the range 0.9967-0.9997. The limits of detection (S/N = 3) for all analytes were 0.0002-0.0003 mg/kg (spirotetramat), 0.0001-0.0003 mg/kg (B-enol), 0.0004-0.0006 mg/kg (B-keto), 0.0004-0.0007 mg/kg (B-mono), 0.0002-0.0006 mg/kg (B-glu), respectively. The limits of quantification (S/N = 10) for all analytes were 0.0006-0.001 mg/kg (spirotetramat), 0.0003-0.001 mg/kg (B-enol), 0.0012-0.0016 mg/kg (B-keto), 0.0012-0.0019 mg/kg (B-mono), 0.0006-0.0013 mg/kg (B-glu), respectively. The method analysis results met the requirements for pesticide residue analysis. And this method is applicable to simultaneous detection of spirotetramat and its four metabolites in spinach, soil and water.关键词
液相色谱-串联质谱/菠菜/螺虫乙酯/代谢物/QuEChERS/固相萃取/残留Key words
liquid chromatography-tandem mass spectrometry (LC-MS/MS)/Spinacia oleracea L./spirotetramat/metabolites/QuEChERS/solid phase extraction/residue分类
农业科技引用本文复制引用
孟志远,任莉,宋玥颐,徐志英,陈小军..液相色谱-串联质谱法同时测定菠菜、土壤及水体中螺虫乙酯及4种代谢物残留[J].农药学学报,2017,19(4):482-490,9.基金项目
江苏省重点研发计划项目 (现代农业)(BE2015354) （现代农业）
扬州市科技计划项目 (YZ2015029) （YZ2015029）
扬州市科技计划 (产学研合作专项)(YZ2016252). （产学研合作专项）
